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Method for preparing vanadium trioxide from vanadium-containing solution

A vanadium trioxide solution technology, applied in the field of vanadium chemical industry, can solve the problems of low cost, difficult reduction reaction, short process flow, etc., and achieve low production cost, reduced reaction temperature and partial pressure of hydrogen, and short process flow Effect

Inactive Publication Date: 2017-12-05
HEBEI IRON AND STEEL
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Problems solved by technology

[0009] In view of the problems existing in the prior art, the present invention provides a method for preparing vanadium trioxide from a vanadium-containing solution, which solves the technical problem that the reduction reaction is difficult to carry out due to the generation of sodium hydroxide in the hydrogen reduction process of vanadate, The reduction efficiency of vanadate is improved, and the vanadium trioxide product with a purity greater than 99% is obtained. At the same time, the generation of ammonia nitrogen wastewater is effectively avoided. It has the characteristics of short process flow, clean production, high-end products, and low cost. It is suitable for industrialization promotion

Method used

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  • Method for preparing vanadium trioxide from vanadium-containing solution

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Effect test

Embodiment 1

[0052] (1) Pass CO into the sodium pyrovanadate solution containing vanadium concentration of 46g / L 2 and H 2 , at 120°C, CO 2 Partial pressure 0.5MPa, H 2 Under the conditions of partial pressure 2MPa and stirring speed of 500r / min, react in a high-temperature and high-pressure reactor for 2 hours, filter after the reaction is completed, and obtain vanadium trioxide solid and separation liquid;

[0053] (2) drying the vanadium trioxide solid obtained in step (1) at 105° C. under a nitrogen atmosphere to obtain a vanadium trioxide product;

[0054] (3) At 15°C, feed CO into the separation liquid obtained in step (1) 2 Carry out acidification reaction, stir at a speed of 200r / min, the pH value of the reaction end point is 8.0, filter and separate sodium bicarbonate crystals and filtrate after reacting for 1.5h; return the obtained filtrate to the sodium vanadate solution preparation process for recycling.

[0055] After testing, the reduction rate of vanadate in this embodi...

Embodiment 2

[0057] (1) Pass CO into the sodium pyrometamate solution containing vanadium concentration of 32g / L 2 and H 2 , at 150°C, CO 2 Partial pressure 1MPa, H 2 Under the condition of partial pressure of 2.5MPa and stirring speed of 700r / min, react in a high-temperature and high-pressure reactor for 3 hours, filter after the reaction is completed, and obtain vanadium trioxide solid and separation liquid;

[0058] (2) drying the vanadium trioxide solid obtained in step (1) at 280° C. under a nitrogen atmosphere to obtain a vanadium trioxide product;

[0059] (3) At 25°C, feed CO into the separation liquid obtained in step (1) 2 Perform acidification reaction, stir at a speed of 250r / min, the pH value of the reaction end point is 8.2, filter and separate sodium bicarbonate crystals and filtrate after reacting for 2 hours; return the obtained filtrate to the sodium pyrovanadate solution preparation process for recycling.

[0060] After testing, the reduction rate of vanadate in this...

Embodiment 3

[0062] (1) To the vanadium concentration of 25g / L containing sodium metavanadate solution into the CO 2 and H 2 , at 100°C, CO 2 Partial pressure 0.8MPa, H 2 Under the condition of partial pressure of 2.2MPa and stirring speed of 350r / min, react in a high-temperature and high-pressure reactor for 3 hours, and filter after completion of the reaction to obtain vanadium trioxide solid and separation liquid;

[0063] (2) drying the vanadium trioxide solid obtained in step (1) at 200° C. under an argon atmosphere to obtain a vanadium trioxide product;

[0064] (3) At 20°C, feed CO into the separation liquid obtained in step (1) 2 Carry out acidification reaction, stir at a speed of 100r / min, the pH value of the reaction end point is 7.8, filter and separate sodium bicarbonate crystals and filtrate after reacting for 1 hour; return the obtained filtrate to the sodium metavanadate solution preparation process for recycling.

[0065] After testing, the reduction rate of vanadate i...

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Abstract

The invention relates to a method for preparing vanadium trioxide from a vanadium-containing solution. The method comprises the steps of introducing CO2 and H2 into the vanadium-containing solution, carrying out a reaction under heated and pressurized conditions, and carrying out solid-liquid separation after the reaction is completed, thereby obtaining solid vanadium trioxide and a separated solution. According to the method disclosed by the invention, the gas mixture of CO2 and H2 is adopted to react with the vanadium-containing solution, so that the technical problem that a reduction reaction is difficult to carry out due to the fact that sodium hydroxide is produced in a hydrogen gas reduction process of vanadate is solved; the efficiency of reduction of the vanadate is increased, and the vanadium trioxide product with the purity higher than 99% is obtained; and meanwhile, the generation of ammonia nitrogen wastewater is effectively avoided, the cyclic utilization of water resources is achieved, and the aim of zero wastewater emission is achieved. The method has the characteristics of short process flow, high production efficiency, high-end product, environment-friendliness, low cost and the like and is applicable to industrialized popularization.

Description

technical field [0001] The invention relates to the field of vanadium chemical industry, in particular to a method for preparing vanadium trioxide from a solution containing vanadium. Background technique [0002] Vanadium oxides are mainly used in the production of alloys, colorants for ceramic printing and dyeing, electrolytes for all-vanadium redox flow batteries, sulfuric acid and catalysts for petrochemical industries such as metallurgy, electronics, dyes, energy, and chemicals. Vanadium oxides are mainly vanadium pentoxide (V 2 o 5 ), vanadium trioxide (V 2 o 3 ) and vanadium dioxide (VO 2 ), etc., different oxides have different preparation processes. [0003] In the vanadium metallurgical industry, vanadium pentoxide is used as the primary product of vanadium. The vanadium-containing minerals undergo hydrometallurgy to obtain a vanadium-containing solution. The impurity elements in the solution are removed by chemical removal, and then the vanadium pentoxide is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02C01D7/00
CPCC01G31/02C01D7/00C01P2006/80
Inventor 常福增陈华李兰杰黄山珊高玲玲
Owner HEBEI IRON AND STEEL
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